XXIX. METHODS FOR THE ANALYSIS OF DRUGS. PROVISIONAL. 



[See Appendix, p. 258, for methods for alkaloids.] 



1. Assay of Opium. 



(a) REAGENTS. 



(1) Ammonia water, 3.5 cc. 



(2} Alcohol, ether, distilled water, and lime water in sufficient quantities. 



(b) DETERMINATION. 



Introduce 10 grams of opium (which if fresh, should be in very small pieces, and 

 if dry, in very fine powder) into an Erlenmeyer flask having a capacity of about 300 

 cc, add 100 cc of distilled water, stopper the flask and agitate it every ten minutes 

 (or continuously in a mechanical shaker) during three hours. Then pour the con- 

 tents as evenly as possible upon a wetted filter having a diameter of 12 cm, and, 

 when the liquid has drained off, wash the residue with distilled water, carefully 

 dropped upon the edges of the filter and its contents, until 150 cc of filtrate have 

 been obtained. Then carefully transfer the moist opium back to the flask by means 

 of a spatula, add 50 cc of distilled water, agitate it thoroughly and repeatedly dur- 

 ing fifteen minutes, and return the whole to the filter. When the liquid has been 

 drained off, wash the residue as before, until the second filtrate measures 150 cc, 

 and finally collect about 20 cc more of a third filtrate. Evaporate carefully in a 

 tared dish, first, the second filtrate to a small volume, then add the first filtrate, 

 rinsing the vessels with the third filtrate, and continue the evaporation until the 

 residue weighs 14 grams. Rotate the concentrated solution about in the dish until the 

 rings of extract are redissolved, pour the liquid into a tared Erlenmeyer flask, hav- 

 ing a capacity of about 100 cc, and rinse the dish with a few drops of water at a 

 time until the entire solution, after the rinsings have been added to the flask, weighs 

 20 grams. Then add 10 grams (or 12.2 cc) of alcohol, shake the flask well, add 25 cc 

 of ether, and repeat the shaking. Now add the ammonia water from a graduated 

 pipette or burette, stopper the flask with a sound cork, shake it thoroughly during 

 ten minutes, and then set it aside, in a moderately cool place, for at least six hours, 

 or overnight. 



Remove the stopper carefully, and should any crystals adhere to it, brush them 

 into the flask. Place in a small funnel two rapidly acting filters, of a diameter of 

 7 cm, plainly folded, one within the other (the triple fold of the inner filter being 

 laid against the single side of the outer filter), wet them well with ether, and de- 

 cant the ethereal solution as completely as possible upon the inner filter. Add 10 

 cc of ether to the contents of the flask, rotate it, and again decant the ethereal layer 

 upon the inner filter. Repeat this operation with another portion of 10 cc of ether. 

 Then pour the liquid in the flask into the filter, in portions, in such a way as to 

 transfer the greater portion of the crystals to the filter, and when the liquid has 

 passed through, transfer the remaining crystals to the filter by washing the flask 



U. S. Pharmacopoeia, 8 Rev., p. 329. 



201 



